固相萃取-气相色谱－三重四级杆质谱法测定蔬菜中五氯硝基苯和百菌清残留量

Determination of pentachloronitrobenzene and chlorothalonil residues in vegetables by solid phase extraction-gas chromatography triple quadrupole mass spectrometry

中文关键词:  固相萃取  五氯硝基苯和百菌清  气相色谱－三重四级杆质谱联用仪

英文关键词:solid phase extraction  pentachloronitrobenzene and chlorothalonil  gas chromatography triple quadrupole mass spectrometer

中文摘要:

      目的 建立固相萃取-气相色谱－三重四级杆质谱法测定蔬菜中五氯硝基苯和百菌清残留量的检测方法。方法 样品采用正己烷溶剂提取, 串联Florisil-Carb固相萃取小柱净化, 采用多重反应监测(multiple reaction monitoring, MRM)模式检测, 内标法进行定量。结果 五氯硝基苯和百菌清的平均回收率分别在78.7%~91.6%、80.2%~90.8%之间; 检出限(S/N=3)为0.005 mg/kg和0.004 mg/kg。结论 该方法具有灵敏度高、分离效果好、重复性好的特点, 适用于大批量蔬菜样品中五氯硝基苯和百菌清杀菌剂残留检测的要求。

英文摘要:

      Objective To establish a method for the determination of quintozene and chlorothalonil residues in vegetables by solid phase extraction-gas chromatography-triple quadrupole mass spectrometry. Methods The samples were extracted with N-hexane solvent, purified with Florisil-carb solid phase extraction column in series, detected by multiple reaction monitoring (MRM) mode, and quantified by internal standard method. Results The average recoveries of quintozene and chlorothalonil were 78.7%–91.6% and 80.2%–90.8%, and the detection limits (S/N=3) were 0.005 mg/kg and 0.004 mg/kg, respectively. Conclusions This method has the characteristics of high sensitivity, good separation effect and good repeatability. It is suitable for the detection of pentachloronitrobenzene and chlorothalonil residues in a large number of vegetable samples.